GOST 22720.1-77

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

gost-227201-77.pdf (1.86 MiB)
ГОСТ 22720.1-77

GOST 22720.1−77 Rare metals and alloys on their basis. Methods of determination of oxygen, hydrogen, nitrogen and carbon (with Amendments No. 1, 2)

GOST 22720.1−77*

Group B59

STATE STANDARD OF THE USSR

RARE METALS AND ALLOYS ON THEIR BASIS

Methods of determination of oxygen, hydrogen, nitrogen and carbon

Rare metals and their alloys. Methods for the determination of oxygen, hydrogen, nitrogen and carbon

AXTU 1709*
____________________

* Changed the wording, Rev. N 2.

Date of introduction 1979−01−01

The decision of the State standards Committee of the Council of Ministers of the USSR from September 29, 1977 N 2341 introduction installed from 01.01.79

Proven in 1983 by the Decree of Gosstandart from 27.07.83 3511 N validity extended to 01.01.89**

________________

** Expiration removed by Protocol No. 3−93 Interstate Council for standardization, Metrology and certification. (IUS No. 5/6, 1993). — Note the manufacturer’s database.

* REISSUE. November 1983, Change 1, approved in July 1983; Post. 3512 N from 27.07.83 (IUS N 11, 1983).

The Change N 2 approved and put into effect by the Decree of the USSR State Committee for standards from 02.03.88 N 427 with 01.01.89

Change No. 2 made by the manufacturer of the database in the text IUS N 5, 1988

This standard applies to zirconium, hafnium, vanadium, niobium, tantalum, molybdenum, tungsten, rhenium, gallium, indium, yttrium, all rare-earth metals, fluorides of rare-earth metals, and binary alloys, whose composition is given in table.1 GOST 22720.0−77, and establishes methods of vacuum extraction for the determination of oxygen, hydrogen, nitrogen and carbon.

The standard does not specify methods for the determination of hydrogen in metals and alloys with a melting point of ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1200 °C.

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 22720.0−77.

2. APPARATUS, REAGENTS AND SOLUTIONS

«Installation «Giredmet-911М1», which is supplemented by the oxygen supply system in an extraction part (damn.1) to determine the content of gas-forming impurities in metals.

ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2)

1 — extraction oven; 2 — oxygen cylinder with reducer; 3, 5, 7, 10, 13, 14, 16, 18 — vacuum valves; 4 — bellows vacuum gauge; 6 — feeder; 8, 15 — parachute diffusion pump; 9 — reserve tank; 11 is the oxidation oven; 12 — gauge Mac-Leod; 17 — roughing pump

Damn.1

The installation of «Giredmet C-1403M1» block oxygen supply (Fig.2) to determine the content of gas-forming impurities in metals.

1 — oxygen cylinder with reducer; 2 — bellows vacuum gauge; 3, 15 — vacuum valve; 4 — vacuum the gateway boot device; 5, 9, 11, 13, 17, 18, 19, 22, 24, 25, 26 — small electromagnetic valves; 6, 7 — large solenoid valves; 8, 27 — parachute diffusion pumps, traps; 10 — oxidizing furnace; 12 — reserve tank; 14, 23, 29 — thermocouple manometric lamps; 16 — gauge automatic Mac-Leod; 20 — forevacuum pumps; 21 — foreline trap; 28 — ionization gauge lamp; 30 — extraction furnace

Damn.2

The installation of «Giredmet-911М1», equipped with an extraction oven with hub current.

The installation is complemented by the boot devices of transparent quartz: compression gauges analyzers — scales with divisions of 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) Torr.

Tubular resistance furnace for heating of samples in the boot device. Main oven features:


inner diameter	(26±0,5) mm;
length	(140±10) mm;
the material of the heater	nichrome;
the heater resistance	50−100 Ohms;
wire diameter	0.4−0.8 mm;
the limits of temperature regulation	300−1100 °C.

Allowed to use other equipment, not inferior to the main analytical parameters (repeatability, limit of detection, the void, the amendment in the reference experiment, the temperature of the crucible) the above devices.

Crucibles, screens and other parts from graphite grade GSOC or MGOC.

Alumina laboratory crucibles.

Bars and strip Nickel brand H1 or H2, purified in a vacuum.

Copper wire according to GOST 1535−71*.
______________
* On the territory of the Russian Federation GOST 1535−2006. — Note the manufacturer’s database.

Platinum affilirovannaja brand PLA-1 according to GOST 12341−81*.
______________
* On the territory of the Russian Federation GOST 31290−2005. — Note the manufacturer’s database.

The granulated copper oxide according to GOST 16539−79.

Grease vacuum tubes.

Nitric acid GOST 4461−77.

Hydrofluoric acid according to GOST 10484−78.

Ether ethyl technical GOST 6265−74 or H. h

Rectified ethyl alcohol GOST 18300−87.

Oxygen gaseous technical GOST 5583−78.

Nitrogen liquid technical, GOST 9293−74.

Distilled water GOST 6709−72.

Tin granular brand 01 or 02 according to GOST 860−75.

Mercury brands r0 according to GOST 4658−73.

Vacuum oil VM-4.

Medical absorbent cotton wool GOST 5556−81.

Cotton calico GOST 11680−76.

Methane.

Potassium chronologicly according to GOST 4459−75.

Sulfuric acid according to GOST 4207−75.

(Changed edition, Rev. N 1, 2).

3. PREPARATION FOR ASSAY

3.1. Sample preparation, capsules, bath material to the analysis.

The analysis is carried out on two samples, the mass of which is selected in accordance with table.1. Samples are prepared as follows.

Table 1


Mass fraction of impurities, %	The sample mass, g, in determining
	oxygen	carbon	nitrogen	hydrogen
1·10-2·10	-	3	-	-
2·10-5·10	-	2−3	2−3	-
5·10-1·10	2,3	1,5	1,5	-
1·10-5·10	1,5	0,5−1,0	0,5−1,0	-
1·10-1·10	1,0−0,8	1,0−0,5	0,5−0,4	1,1−0,9
1·10-5·10	1,0−0,8	0,5−0,4	0,4−0,3	0,9−0,8
5·10 — 1·10	0,8−0,5	0,4−0,3	0,3−0,2	0,8−0,5
1·10-3·10	0,6−0,3	0,3−0,2	0,3−0,2	0,5−0,2
3·10-1·10	0,3−0,1			0,2−0,1
SV. 1·10	0,1−0,05			0,1−0,005

Powder or foil (samples in the form of chips do not analyze) with a thickness of ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 50 microns was charged into a mold (Fig.3) compressed tablets of 0,1−0,5 g.

1 — ferrule; 2 — insert-matrix; 3 — upper punch; 4 — the lower punch

Damn.3

From ingots, sheets, rods, etc. selected compact samples in accordance with the standards and normative and technical documentation for these products. The samples taken from the ingots, samples of foil and wire thickness of 0.1 mm is etched under the conditions shown in table.1A.

Table 1A


The analyzed material	The composition of the Etchant	The etching temperature, °C	The time of etching, min.
Niobium, silicon	HF:HNО=1:3	25	2
Molybdenum	HF:HNО=6:1, rinsing in a solution of bichromate of	25	1
Rhenium	HF:HNО=6:1, rinsing in a solution of bichromate of	50	2
Hafnium, zirconium	HF:HNО=1:5	25	1
Vanadium	HNО:NO=1:1	25	2

After etching samples were washed in distilled water and ethanol (10 cm ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) of alcohol to one sample). In determining the carbon rinsing in alcohol is excluded. The washed samples are transferred only with clean tweezers. Samples stored in closed buksh to avoid contamination of the surface.

Bath material (copper, Nickel, platinum) cut into pieces weighing 1.5−2 g, washed in alcohol and air dried. As a passivating sublimate used tin, melted in a graphite crucible at a pressure of 0.133 PA (1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) Torr). Pieces of tin 0.3−0.4 g washed in alcohol and air dried.

Capsule (Fig.4) are machined from vacuum melting of Nickel with a mass fraction of oxygen <1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) %, annealed in a current of hydrogen or in a vacuum at (1000±50) °C for 1 h.

Damn.4

After loading the sample in the capsule edge of the latter is clamped with pliers or in a vise, clamping the surface of which is pre-degreased. Samples in capsules are transferred only with clean tweezers.

When determining nitrogen as the bath material used bar sections of Nickel with a diameter of 12 mm and a length of 25 mm. in the determination of carbon — the same bar sections of Nickel and pieces of carbonyl iron by weight, of 0.1−1.0 g of the Material of the bath before loading into the crucible was washed with alcohol and air dried.

(Changed edition, Rev. N 1).

4. ANALYSIS

4.1. Definition of oxygen by the method of reductive melting in a vacuum

The method of reductive melting in a vacuum to determine the oxygen is the following: the sample is the analyzed metal is thrown into a graphite crucible vacuum furnace (melting of water) or in the melt (bath) and another metal (iron, Nickel, platinum, etc.), saturated with carbon. The sample melts or dissolves in the bath. Contained in the sample of the oxygen connects to the carbon emitted in the gas phase in the form of carbon monoxide and enters the detector where it is quantification.

4.1.1. The determination of oxygen in niobium, molybdenum and alloys of niobium-molybdenum and niobium-vanadium fusion of water (with mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10%).

The analysis is carried out on the «Giredmet-1403М1» (see the devil.2). Extraction oven Assembly is shown in hell.5. Before analysis the crucible is degassed at a temperature of (2400±50) °C for 30−60 min. the End of the degassing is characterized by the correction control experience ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 3·10% oxygen per 1 g sample for 2 min at assay temperature (2350±50) °C.

1 — water-cooled quartz bulb; 2 — quartz funnel; 3 — the first graphite screen; 4 — graphite microtidal; 5 — second graphite screen; 6 — graphite the holder

Damn.5

The extraction time is 2 min. the Definition of amendments the reference experiment carried out before analysis of each sample in the following order. At least 5 minutes before the start of gas extraction from wet-process kiln transfer valve to its original position (valves 7, 13 is closed, valves 6, 9, 11 and the valve 15 is opened); drain the lock chamber the roughing pump; open the valve of the gateway is 1.5−2 turns, raise the Dewar with liquid nitrogen to the process of the oxidation furnace 10; 10−20 with open valve 7, close the valves 6 and 9, a stopwatch and 15 seconds close the valve of the gateway; after 2 minutes close the valve 7, opens the valve 6. After separation of the gas mixture (switch vacuum gauge in position LT-2) open the valve 9 to evacuate the gas (nitrogen) from the analytical system; closing the valve 9 down the Dewar with liquid nitrogen, and replace it with a Dewar filled with alcohol cooled to minus 60−70 °C, and at the end of the defrosting of carbon dioxide measured CO pressure ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) gauge automatic Mac-Leod 16; open the valve 9 and warm the process of the oxidation furnace.

During the evacuation of gases from the analyzer through an airlock upload another sample, is pumped out of the gateway in fore-vacuum pump, then open the valve the gateway for 1.5−2 turns. After evacuation of gases from the analyzer, the device is ready for the next analysis (valves 6 and 9 are closed, 7 is open). Once you start the stopwatch the handle of the valve is the gateway turn counterclockwise until until the sample drops into the crucible. Following this, the valve of the airlock closed. Further operations are performed in the same order as in the definition of amendments the reference experiment.

Analysis of a series of samples in a single crucible lead until, until the mass of the melt in the crucible does not exceed 10 g.

4.1.1. The determination of oxygen in niobium and molybdenum, the melting temperature of water with the use of the current hub (if the mass fraction of oxygen 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) %)

The analysis is carried out on the «Giredmet-911М1», equipped with an extraction oven with hub current. Before analysis the crucible is degassed at a temperature of (2400±50) °C for 25−30 min. the End of the degassing is characterized by the correction control experience not more than 3 mg of oxygen per 1 min.

Set operating temperature:

(2300±50) °C — for analysis of molybdenum,

(2400±50) °C — for analysis of niobium.

Throw into the crucible a piece of pure oxygen molybdenum (niobium), containing oxygen not more than 0.001%, weight 0.5−1 g check the correct installation operating temperature (the melting time of the sample does not exceed 15 C).

The extraction time is 1 min. the Definition of amendments the reference experiment carried out before analysis of each sample in the following order. At least 2 minutes before the start of gas extraction in the extraction furnace, convert the faucet installation (DWG.1) to its original position, namely, the valve 7 in the position of pumping, valve 16 and valve oxidizing furnace 11 is opened, valve 10 is closed. Then raise the Dewar with liquid nitrogen to the process of the oxidation furnace through 10−20 transferred from the crane to the position of «pumping», close the valve 16 and include a stopwatch. After 1 min transfer crane 7 to «pumping» and watch the end of the process of separation of gas mixtures according to the indications of the vacuum gauge of the analytical system; open the valve 16 to evacuate the gas from the analyzer, close the valve 16; replacing the vessel with liquid nitrogen in a vessel with ethanol, chilled to minus 70 °C, and at the end of the defrosting of carbon dioxide measured CO pressure ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) gauge Mack-Leod 12; open the valve 16.

After the evacuation of gas from the analyzer unit is ready for selecting the next batch of gas. Sample analysis is carried out in the same manner as the definition of amendments the reference experiment.

Analysis of samples within the crucible continues until, until the mass of the melt in the crucible will not exceed 9 g.

4.1.1 b. A comprehensive determination of oxygen in niobium and hafnium (when the mass fraction of oxygen in niobium is more than 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) %, hafnium — more than 3·10%).

The analysis is carried out on the «Giredmet-911М1», equipped with a hub of current, or on the «Giredmet-1403М1». In the horizontal process of the loading device is placed the analyzed material in the following order:

pure niobium electron beam melting a total mass of 1.5 g;

a sample of hafnium by weight not more than 0.3 g;

samples of niobium with a total mass of 1 g;

a sample of hafnium by weight not more than 0.3 g.

The total mass of the samples does not exceed 12 g in the ratio of the mass of niobium by weight of hafnium of not less than 3:1.

Before analysis the crucible is degassed at a temperature of 2400−2450 °C for 40 min. the End of the degassing is characterized by the correction control experience 10 micrograms of oxygen for 3 min. at assay temperature 2400−2450 °C.

To analyze dropping into the crucible 1.5 g of niobium and check correctness of installation operating temperature (the time of complete melting of 1.5 g of niobium at a temperature of 2400−2450 °C — not more than 15). The degassed melt for two to three minutes, then spend the definition of amendments the reference experiment for 3 min, then analyze a sample of hafnium. Extraction time — 3 min. Then determine the correction reference experiment for 1.5 min, and analyze a sample of niobium with a measurement of the magnitude of amendments the reference experiment before analysis of each sample. The extraction of oxygen from the niobium — 1.5 minutes Measure the correction control experience for 3 min, analyze a sample of hafnium as long as the mass of the melt in the crucible will not exceed 12 g.

4.1.1 Integrated V. determination of oxygen in niobium and Rennie (when the mass fraction of oxygen more than 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) %)

The analysis is carried out on the «Giredmet-911М1», equipped with concentrate current or at «Giredmet-1403М1». In the horizontal process of the loading device is placed the analyzed material in the following order:

pure niobium with a total mass of 1.5 g;

sample of rhenium by weight not more than 0.5 g;

the sample of niobium with a total mass of 1 g;

sample of rhenium by weight not more than 0.5 g… etc.

The total mass of the samples does not exceed 12 g in the ratio of the mass of niobium by weight of rhenium is at least 2:1.

Before analysis the crucible is degassed at a temperature of 2400−2450 °C for 40 min. the End of the degassing is characterized by exposures in the reference experiment 3 mg of oxygen per 1 min. at assay temperature 2400−2450 °C for 40 min.

The analysis is carried out as specified in clause 4.1.1 b. The extraction of oxygen from the niobium and rhenium, and time determine the amount of amendments the reference experiment, is 1 min.

Analysis of samples in one crucible leads to until the mass of the melt in the crucible will not exceed 12 g.

4.1.1 g. the Determination of oxygen in niobium, molybdenum and alloys of niobium-molybdenum melting temperature of water pre-treatment surface samples (with a mass fraction of oxygen from 5·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) to 1·10%).

The analysis is carried out on the «Giredmet-1403М1» as specified in clause 4.1.1, or on the «Giredmet-911М1» as specified in clause 4.1.1.

Samples after etching is placed in a quartz boot device, install, vacuum and carry out degassing of the graphite crucible. Degassing time 25−30 min., temperature (2400±50) °C. the End of the degassing is characterized by the correction control experience not more than 3 mg of oxygen per 1 min. Difference between two consecutive measurements amendments the reference experiment should not exceed 0.3 micrograms of oxygen.

After degassing, the heating of the crucible off, the extraction system through a leak valve is supplied methane to reach the pressure (80±10) Thor and the boot device is heated by the tubular furnace for 10 min at a temperature of: molybdenum — (1000±50) °C; for niobium — (1100±50) °C. Then the vacuum extraction system and when you reach a pressure of 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) tor remove the tube furnace.

When heating is pyrolysis of methane, in which the sample surface is cleaned of sorbed oxygen and covered with a protective layer of pyrocarbon, preventing secondary adsorption of oxygen on the samples.

In the cooling process of the samples includes the heating of the crucible and degassed it for 10 min.

In the analysis of niobium in the temperature of the crucible is adjusted to (2200±50) °C, discard the sample and maintain it at this temperature for 2 min. Then transfer valves (taps) of the unit (Fig.1 and 2) to analyze, raise the temperature of the crucible up to (2400±50) °C. the extraction Time (from the moment of complete melting of the sample) 1 min By the end of the extraction process is carried out the measurement of the amendments the reference experiment for a time equal to the exposure time of the sample at the temperature of analysis. After that reduce the temperature of the crucible up to (2200±50) °C and carry out the analysis of the next sample in the same order.

In the analysis of the temperature of the molybdenum crucible was adjusted to (2300±50) °C. the extraction Time (from the moment of complete melting of the sample) 1 min By the end of the extraction process is carried out the measurement of the amendments the reference experiment for a time equal to the exposure time of the sample at the temperature of analysis. The analysis of the next sample is carried out in the same manner.

Analysis of a series of samples of niobium or molybdenum in one lead to the crucible until the mass of melt does not exceed 12 g.

4.1.1 a-4.1.1. (added, Rev. N 1).

4.1.2. The determination of oxygen in vanadia, molybdenum, tungsten, Rennie and alloys, vanadium-niobium, vanadium-molybdenum, vanadium-tantalum, vanadium-tungsten, molybdenum-rhenium, tungsten-rhenium, tungsten-tantalum smelting the Nickel in the bath (when the mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10%)

The analysis lead to the installation of «Giredmet-1403М1» (see the devil.2) or «Giredmet-911М1» (see the devil.1). Extraction oven Assembly is shown in hell.6. Before analysis the crucible is degassed at (2000±50) °C for 1.5−3 hours Then reduce temperature to 1000−1200 °C and dumped into the crucible Nickel segments of the rod with a total mass of 8−10 g. Raise the temperature of the crucible up to (1700±50) °C and the melt is degassed for 10−15 min. the End of the degassing is characterized by the correction control experience ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 3·10% oxygen per 1 g of the sample for 5 min at assay temperature (1700±50) °C.

1 — water-cooled quartz bulb; 2 — quartz funnel; 3 — graphite screen; 4 — graphite crucible

Damn.6

The extraction time is 5 min. To amend the result of the analysis of the control experiment is performed before analysis of each sample. The order of actions while working on the «Giredmet-1403М1» specified in item 4.1.1.

On the «Giredmet-911М1» (see the devil.1) the definition of amendments to the control of experience is determined in the following order. At least 5 minutes before the start of gas extraction from wet-process kiln transfer cranes to its original position (valve 7 in the position of pumping, valve 16 and valve oxidizing furnace 11 is opened, valve 10 is closed), raise the Dewar with liquid nitrogen to the process of the oxidation furnace; 10−20 with transfer valve 7 at position «pumping», close the valve 16 and include a stopwatch; after 5 min, transfer valve 7 in the position of pumping and watching the end of the process of separation of gas mixtures according to the indications of the vacuum gauge of the analytical system; open the faucet 16, evacuating gas from the analyzer; close the valve 16, replace the vessel with liquid nitrogen in a vessel with ethanol, chilled to minus 60−70 °C, and at the end of the defrosting of carbon dioxide measured pressure FROM ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) the pressure gauge Mack-Leod 12; open the valve 16 and warm the process of the oxidation furnace.

After the evacuation of gas from the analyzer unit is ready for selecting the next batch of gas. The analysis of the sample are in the same order as the definition of amendments the reference experiment.

In one crucible you can perform 5−10 samples weighing up to 5 g in the ratio of the mass of the bath to the sample mass (7−10):1. After analysis of each sample in the bath you need to add 3−5 g of Nickel.

4.1.2. The determination of oxygen in metal vanadii and alloy BB-8 fusion in a tin bath (with a mass fraction of oxygen more than 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) %)

The analysis is carried out on the «Giredmet-911М1» or «Giredmet-1403М1». Before analysis the crucible is degassed at a temperature of (2000±50) °C for 2−3 h.

The end of the degassing is characterized by the correction control experience less than 3 mg of oxygen for 3 min. at assay temperature (1800±30) °C.

Determination of amended reference experiment is carried out as specified in clause 4.1.2. Then turn off the heat and after cooling the crucible, reset it to 0.8−1 g of tin. Bring the crucible temperature to (1800±30) °C, increasing the anode current of the oscillating tube for 4 min 2 min repeat the measurement of the amendments the reference experiment.

Analyze the first sample. The extraction time is 3 minutes at a temperature of (1800±30) °C.

Carry out the measurement of the amendments the reference experiment.

For 30 s prior to analysis of the second sample is thrown into the crucible of 0.3−0.4 g of tin.

After the analysis of the second sample is carried out the measurement of the amendments the reference experiment; 30 seconds before the analysis of the third sample is thrown into the crucible of 0.3−0.4 g of tin… etc.

Within the crucible allowed the analysis of up to 20 samples with a total mass up to 10 g.

(Added, Rev. N 1).

4.1.3. The determination of oxygen in niobium, vanadiu, tantalum, molybdenum and binary alloys of these elements, with the exception of alloys with titanium, zirconium, chromium, aluminium and germanium, by melting in a platinum bath (when the mass fraction of oxygen of ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 5·10%)

The analysis is carried out on the «Giredmet-1403М1» (see the devil.2) or «Giredmet-911М1» (see the devil.1). Extraction oven Assembly, see hell.6.

Before analysis the crucible is degassed at (2000±50) °C for 2−3 hours Then reduce the temperature to 1500−1600 °C and dumped into the crucible pieces of platinum with a total weight of 7−8 g. Raise the temperature of the crucible up to (1900±50) °C and Degas the melt 10 min.

The end of the degassing is characterized by the correction control experience 2·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) % oxygen per 1 g of the sample for 5 min at assay temperature (1900±50) °C.

Further analysis are as indicated in the claims.4.1.1 and 4.1.2. The ratio of the mass of the bath to the mass of the analyte support is equal to (8−10):1. With this goal in front of each definition in the pot add appropriate amount of platinum. The total mass of the analyzed material in one crucible should not exceed 7 g.

4.1.4. The determination of oxygen in niobium, tantalum and their binary alloys, except alloys with titanium, zirconium, aluminum and germanium, melting in the Nickel bath and the Nickel capsules (when the mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 2·10%)

The analysis is carried out on the «Giredmet-1403М1» (see the devil.2) or the installation of «Giredmet-911М1» (see the devil.1). Extraction oven Assembly is shown in hell.6.

Before analysis the samples are loaded into capsules (see the devil.4). The crucible is degassed at (2000±50) °C for 1.5−2 hours Then reduce temperature to 1000−1200 °C and dumped into the crucible Nickel segments of the rod with a total mass of 4−5 g. Raise the temperature of the crucible up to (1700±50) °C and the melt is degassed for 10−15 min.

The end of the degassing is characterized by the correction control experience ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 5·10% oxygen (without the capsules) or 1·10% oxygen (with capsule) per 1 g of the sample for 5 min at assay temperature (1700±50) °C. Empty capsules analyzed before the first and last samples. Further analysis are as indicated in the claims.4.1.1 and 4.1.2. The ratio of the mass of the bath to the mass of the analyte support is equal to (7−10):1 (due to the weighted capsules and, if necessary, Supplement pieces of Nickel). The total mass of the analyzed material in one crucible should not exceed 5 g.

4.1.5. The determination of oxygen in zirconium, hafnium and their binary alloys and also in alloys vanadium-zirconium, vanadium-aluminum, vanadium-chromium, niobium-aluminum, niobium-titanium, niobium-germanium by melting in a Nickel bath and Nickel capsules with the use of tin (in mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10%)

The analysis is carried out on the «Giredmet-1403М1» (see the devil.2) or on the «Giredmet-911М1» (see the devil.1). Extraction oven Assembly is shown in hell.6.

Before analysis the samples are loaded into capsules (see the devil.4). The crucible is degassed at a temperature of (2100±50) °C for 3 hours Then turn off the heat and after 2 minutes throw into the crucible 1 g of tin and 4−5 g of Nickel. Turn up the heat, raise the temperature of the crucible up to (1900±50) °C (alloys vanadium-chromium and niobium-germanium — (1700±50) °C and the melt is degassed for 10−15 min. the End of the degassing is characterized by the correction control experience ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 3·10% oxygen (without capsule), or 4·10% oxygen (with capsule) per 1 g of the sample for 5 min at assay temperature (1900±50) °C. Empty capsules analyzed before the first and last samples. After analyzing the first empty capsules dropping into the crucible and 0.3 g of tin, conduct measurement amendments the reference experiment and then analysis of the sample. Further drop in the molten tin before each definition. Further analysis are as indicated in the claims.4.1.1 and 4.1.2. The ratio of the mass of the bath to the mass of the analyte support is equal to (10−15):1. The total mass of the analyzed material in one crucible should not exceed 2.5 g.

4.1.6. Determination of the oxygen content in yttria, rare earth metals and their binary alloys by melting in a copper-Nickel bath (when the mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10%)

The analysis lead to the installation of «Giredmet. -911М1» (see the devil.1). The extraction furnace shown on the devil.7. The graphite cap 5 (see the devil.7) molybdenum wire 6 attached to the steel core, the core moving magnet and serves for lifting and lowering of the lid 5 of the crucible 3.

1 — water-cooled quartz bulb; 2 — the first graphite screen; 3 — graphite crucible; 4 — the second graphite screen; 5 — graphite cover; 6 — molybdenum wire of diameter 0.8−1 mm; 7 — quartz funnel

Damn.7

Graphite parts for extraction of the furnace: the first graphite screen — damn.8, the graphite crucible is crap.9, the second graphite screen — damn.10, a graphite lid — damn.11, quartz funnel — shit.12.

Damn.8

Damn.9

Damn.10

Damn.11

Damn.12

Allowed to use the plant «Giredmet-1403М1» (see the devil.2), which gateway replaced the vacuum glass or quartz boot device, the same boot device installation «Giredmet-911М1».

Before analysis the samples are loaded into a Nickel capsule, differing from that shown on the devil.4 the fact that the drilling depth is 4.5 and 7.5 mm. (When working with a weighted capsules occurs, although short-lived, but unwanted in this case, the cooling of the melt). Along with a sample of each capsule is placed a piece of tin with a mass of 0.3 g and a mass fraction of oxygen <1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) %, and before the capsule loading device is a piece of Nickel weighing 1.5 g

Nickel previously degassed by the same method as the capsule. In two capsules (first and last) provide only a tin (0.3 g). The crucible is degassed at (2000±50) °C for 2 hours Then reduce temperature to 1000−1200 °C, dropping into the crucible, the material of the bath 15 g of copper and 15 g of Nickel, the temperature was raised to (1700±50) °C and the melt is degassed for 15−20 min.

The end of the degassing is characterized by exposures in the reference experiment ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10% oxygen (without capsule) or 3·10% oxygen (with Nickel, and tin capsule) per 1 g of the sample for 5 min at assay temperature (1700±50) °C.

After the measurement the amendments in the reference experiment the graphite lift the cover 5 (see the devil.7), drop into the crucible 1.5 g Nickel capsule with a tin (without the sample), close the lid and pump the gas into the analyzer within 5 minutes of Capsule with samples analyzed in the same way, but a piece of Nickel dropped for 20 to capsules. Analysis of the mixture of the extracted gases is carried out as specified in clause 4.1.2. The total mass of the analyzed material in one crucible should not exceed 1.5 g for samarium, europium and 3.0 g for other rare earth metals.

4.1.7. The determination of oxygen in fluorides of rare-earth metal elements and yttrium by melting without bath (with mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10%)

The analysis lead to the installation of «Giredmet-911М1» (see the devil.1). Extraction oven Assembly is shown in hell.13. Graphite cover 8 (see traits.13) through the bushing 12 locks the crucible 5. Cover 8 molybdenum wire 9 is attached to a steel pushrod that moves a magnet and serves for lifting and lowering of the lid 8.

1 — water-cooled quartz bulb; 2 — quartz insert; 3 — graphite holder; 4 — the first graphite screen; 5 — graphite crucible; 6 — graphite reflectors, petals; 7, the second graphite screen; 8 — graphite cover; 9 — molybdenum wire of diameter 0.8−1 mm; 10 — quartz funnel; 11 — graphite pins; 12 — first graphite bushing; 13 — the second graphite sleeve

Damn.13

Graphite and quartz items to the extraction furnace: quartz funnel — shit.14, the graphite holder — features.15, the first graphite screen — damn.16, a graphite crucible crap.17, the graphite reflector petal — hell.18, the second graphite screen — damn.19, graphite cover — damn.20, quartz funnel — shit.21, a graphite pin — damn.22, the first graphite sleeve — hell.23, the second graphite sleeve — hell.24.

Damn.14

Damn.15



Damn.16	Damn.17

Damn.18



Damn.19	Damn.20	Damn.21

Damn.22	Damn.23	Damn.24

Allowed to use the plant «Giredmet-1403М1» in which gateway replaced the vacuum glass or quartz boot device, the same boot device installation «Giredmet-911М1».

The crucible is degassed at (2100±50) °C for 2−3 h. the End of the degassing is characterized by the correction control experience ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 3·10% oxygen per 1 g of the sample for 5 min at assay temperature (1800±50) °C.

Before dropping of the sample in a graphite lid on the crucible UPS and downs, once the sample drops into the crucible. The extraction time is 5 min. the Order of analysis specified in the claims.4.1.1 and 4.1.2. Amendment in the reference experiment is determined before analysis of the next sample.

4.1.8. The determination of oxygen in rare earth metals, yttria and alloys of mischmetal, samarium-praseodymium, gadolinium-samarium method of melting in a bath of rare earth metal fluoride (if the mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 2·10%)

Equipment, the conditions of the degassing crucible and the analysis is in paragraph 4.1.7. In front of each definition the crucible shed 0.4−0.5 g of processed fluoride is one of the rare earth metals (with the exception of the fluorides of samarium and europium) and 0.3 g of tin and degassed 5 min. the Amount of material that is allowed to analyze in a single crucible in a continuous process is 4 g (1 g for samarium and europium). In the analysis of samarium and europium in a crucible along with a tin and a fluoride of rare-earth metals is introduced 0.3 g of indium, and after each definition in an extraction oven let the oxygen to a pressure 0,053−0,067 MPa (400−500 Torr) followed by evacuation and degassing of the crucible at a temperature of 2000 °C to establish the magnitude of the amendment of the control of the experience specified in clause 4.1.7.

4.1.9. Oxygen determination in India, Gaul, and their binary alloys the melting temperature of water (at the mass fraction of oxygen of ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 5·10%)

The analysis is carried out on the «Giredmet-911М1» (see the devil.1). Extraction oven Assembly is shown in hell.25. Graphite cover 6 (see the devil.25) molybdenum wire 7 attached to the steel core, which moves the magnet and serves for lifting and lowering the cover 6 of the crucible 5.

1 — water-cooled quartz bulb; 2 is a quartz insert (see the devil.13); 3 — graphite holder; 4 — graphite screen; 5 — graphite crucible; 6 — graphite cover; 7 — molybdenum wire with diameter 0,8−1 mm

Damn.25

The graphite parts to the extraction furnace: graphite holder — features.26, a graphite screen — damn.27, graphite crucible — damn.28, a graphite cap — hell.29.



Damn.26	Damn.27

Damn.28	Damn.29

Allowed to use the plant «Giredmet-1403М1» in which gateway replaced the vacuum glass or quartz boot device, the same boot device installation «Giredmet-911M1».

The crucible is degassed at (2000±50) °C for 1−1,5 hours the End of the degassing is characterized by exposures in the reference experiment ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10% oxygen for 1 g of sample for 3 min at (1150±50) °C. After the correction of the reference experiment raise a graphite lid 6, dropping the sample into the crucible 5 and close the lid. Operations analysis of a mixture of the extracted gases is carried out as specified in the PP.4.1.1 and 4.1.2, with a measurement amendments the reference experiment prior to each analysis.

4.2. The determination of oxygen by high temperature vacuum heating

Method of high-temperature vacuum heating for the determination of oxygen consists in the following. The sample drop into the graphite crucible vacuum furnace at a temperature of 2000 °C. the oxygen diffuses to the sample surface, where it reacts with gaseous carbon in equilibrium with graphite of the crucible. The resulting carbon monoxide is released in the gas phase and quantitatively determined in the gas analyzer.

4.2.1. The determination of oxygen in niobium, tantalum, molybdenum, tungsten, Rennie and alloys niobium-tungsten, niobium-molybdenum, tantalum-tungsten, molybdenum-rhenium, tungsten-rhenium without melting of the sample (with the mass fraction of oxygen ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 2·10%)

Analyze compact samples with thickness not exceeding 1 mm and samples in powder and foil, pressed, as indicated in sec. 3. The analysis is carried out on the «Giredmet-1403М1» (see the devil.2) or on the «Giredmet-911М1» (see the devil.1). Instead of a stepped graphite crucible (see the devil.6) use a thin-walled crucible (thickness of the bottom and sides of 2 mm). Before analysis the crucible is degassed for 1.5−2 h at (2200±50) °C. the End of the degassing is characterized by exposures in the reference experiment ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10% oxygen for 1 g of sample for 10 min at assay temperature (2000±50) °C.

After dropping the sample into the crucible, carry out the high temperature extraction for 10 minutes For inclusion in the analysis result of the amendment of the control and the experiment is performed before analysis of each sample (as specified in the PP.4.1.1 and 4.1.2). Analysis are in the same order as in the definition of amendments the reference experiment, as long as the total mass of the analyte will not exceed 10 g.

4.3. Determination of carbon

Method for the oxidative melting in a vacuum to determine the amount of carbon is as follows. In the vacuum induction furnace is placed corundum crucible, where the melt of iron-Nickel mixture and saturate the melt with oxygen from the gas phase. The system then creates a vacuum. After degassing the formed carbon-free melt of a Nickel-iron-oxygen. In the melt, dropping the sample of the analyzed metal. Upon dissolution of the sample, the carbon contained therein is oxidized, the reaction products are distinguished in the gas phase. The gas enters the analyzer where it is determined the number.

4.3.1. Determination of carbon in zirconium, hafnium, vanadia, niobium, tantalum, molybdenum, tungsten, Rennie, Gaul, India, yttria, rare earth metals and binary alloys by the method of oxidative melting in vacuum (at a mass fraction of carbon from 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) to 3·10%)

The analysis is carried out on the «Giredmet-911М1» (hell.1) or on the «Giredmet-1403М1» (hell.2). Extraction oven Assembly is shown in hell.30.

1 — water-cooled quartz bulb; 2 — quartz funnel; 3 — the screen is made of Nickel foil with a thickness of 0.1 mm; 4 — outer corundum crucible (bottom diameter 21 mm, top diameter 25 mm, height 45 mm); 5 — inner corundum crucible (bottom diameter 17 mm; top diameter 21 mm, height 125 mm); 6 — filling between the outer and inner crucible of alumina powder; 7 — quartz stand

Damn.30

The outer crucible 4 sleep corundum with grain size of 50−100 µm to a height of 4−5 mm. Powder made from the material of the crucibles. The inner crucible 5 is inserted into the outer, between the walls of the crucible poured corundum powder. Inside the funnel 2 is inserted a screen of Nickel foil, twisted into the shape of a tube. Foil thickness 0.1−0.2 mm. the Outer diameter of the screen equal to the inner diameter of the funnel, the height of the screen is greater than the height of the cylindrical part of the funnel at 40−60 mm. Lower edge of the funnel when installed in an extraction furnace should be 3−5 mm is omitted in the inner crucible. In the inner crucible load 3.5 g of carbonyl iron and cut Nickel rod with a length of 25 mm and a diameter of 12 mm. the Crucible Assembly is mounted on a quartz stand inside 7 of the flask 1 and suspended from the funnel.

When preparing installation to the analysis trap pumping the diffusion pump (see the devil.1) pour 150−200 cm ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) of ethanol and liquid nitrogen or dry ice to bring its temperature to minus 50 °to 70 ° C.

Heating of the material of the bath is initiated when the pressure in the extraction furnace is not more than 0,67 PA (5·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) Torr). The temperature was raised gradually to (900±50) to (1600±50) °C for 15 minutes After melting of the bath and reach the pressure above the melt below 6.7 PA (5·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) Torr) in an extraction furnace oxygen under pressure (0,067±0,0067) MPa [(500±50) Thor] and is kept molten in an oxygen atmosphere for 5−7 min, then oxygen is evacuated, the melt degassed for 15−20 min and repeat the supply of oxygen, followed by aging for 3−5 min. then the temperature was raised to melt (1700±50) °C and is carried out degassing for 1.5−3 h until reaching the value of amendments reference experiment ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 2·10% of carbon per 1 g of the sample in terms of analysis specified in table.2.

Table 2


The analyzed material	Temperature of extraction, °C	Extraction time, min	The highest permissible ratio of the mass of the bath to the mass of the analyte	The mass of the analyte in a single crucible, g
Gallium, indium and their alloys	1500±50	5	5:1	10
Tantalum, niobium, molybdenum, rhenium and their alloys	1700 ±50	7	5:1	10
Vanadium and its alloys	1700±50	5	7:1	7
Zirconium, yttrium, rare earth metals and their alloys	1650±50	3	10:1	5
Hafnium	1800±50	10	20:1	2,5
Tungsten	1800±50	7	7:1	7

The definition of amendments the reference experiment carried out before analysis of each sample.

On the «Giredmet-1403М1» (see the devil.2) the amendment reference experiment is determined in the following order: not less than 5 min prior to the measurement, convert the valve to its original position (valves 7, 13 is closed, valves 6, 9, 11 and valve 15 is open), raise the Dewar with liquid nitrogen to the process of the oxidation furnace 10; 10−20 with open valve 7, close the valves 6 and 9 and a stopwatch; at the end of the gas closing valve 7; at the end of the oxidation process of carbon monoxide to dioxide open valve 9 to evacuate the gas (nitrogen) from the analytical system, close the valve 9, the lower the Dewar with liquid nitrogen, and replace it with a Dewar filled with alcohol cooled to minus 60−70 °C; after thawing, the carbon dioxide measure her blood pressure using the automatic pressure gauge Mack-Leod 16; open the valve 9 and warm the process of the oxidation furnace.

During the evacuation of gases from the analyzer through an airlock upload another sample, is pumped out of the gateway in fore-vacuum pump, then open the valve the gateway for 1.5−2 turns. After evacuation of gases from the analyzer, the device is ready for the next analysis (valves 6 and 9 are closed, 7 is open). Once you start the stopwatch the rotation of the handle gateway dropping the sample into the crucible and the gateway closed.

On the «Giredmet-911М1» (see the devil.1) the amendment reference experiment is determined in the following order: not less than 5 min prior to the measurement, convert the valves to the original position (the valve 7 is in the position of pumping, valve 16 and valve oxidizing furnace 11 is opened, valve 10 is closed), raise the Dewar with liquid nitrogen to the oxidizing process furnace 11; 10−20 with transfer valve 7 at position «pumping», close the valve 16 and include a stopwatch; at the end of the gas transfer valve 7 in the position of pumping; after completion of the oxidation of carbon monoxide to open the valve 16 to evacuate the gas (nitrogen) analyzer; close the valve 16, replace the Dewar vessel with liquid nitrogen in a Dewar filled with alcohol cooled to minus 60−70 °C; after thawing of carbon dioxide measured by the pressure gauge Mack-Leod 12; open the valve 16, the heat process of the oxidation furnace.

After the evacuation of gas from the analyzer unit is ready for selecting the next batch of gas.

Analysis of samples on the «Giredmet-1403М1» and «Giredmet-911М1» are in the same sequence as in the definition of amendments the reference experiment, and continue as long as the total mass of the analyte will not exceed the value specified in table.2. Conditions analysis for specific materials are given in table.2.

4.3.2. Determination of carbon in niobium, molybdenum, silicon pre-treatment of the sample surface (with a mass fraction of carbon from 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) to 1·10%)

The analysis is carried out as specified in clause 4.3.1. Samples after etching is placed in a quartz boot device, installing a vacuum; melt and oxidize in the bath. Before the second oxygen supply boot device heated tubular furnace. The furnace temperature during heating of molybdenum (500±50) °C, niobium and silicon (950±50) °C. after 5 min in an extraction system oxygen at a pressure of (450±5) Thor and kept for 2−3 min. Then vacuum the system and when reaching the pressure of (3−5)·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) tor remove the tube furnace.

Upon heating the sample in an oxygen atmosphere is the removal of surface-sorbing carbon and nitrogen. As a result of oxidation of the surface decreases the probability of secondary adsorption of carbonaceous compounds and nitrogen.

The degassing time is 1.5−2 h. the End of the degassing is characterized by the correction control experience less than 1 µg of carbon. The difference between two consecutive measurements amendments the reference experiment should not exceed 0.1 µg of carbon.

(Added, Rev. N 1).

4.4. Determination of nitrogen

The method of vacuum-melting carbon-free Nickel bath for determination of nitrogen is as follows. The sample dumped into a melt of Nickel in corundum crucible vacuum induction furnace. After dissolution of the sample in the bath, nitrogen is released from the melt to the gas phase and is pumped into the analyzer, which is determined by the amount.

4.4.1. Determination of nitrogen in niobium, the tantalum, vanadii, molybdenum, tungsten, Rennie, zirconium, hafnium, yttria, rare earth metals and their binary alloys, except for alloys with with aluminium, germanium and silicon by vacuum extraction into carbon-free melt of Nickel (at a mass fraction of nitrogen from 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) to 3·10%)

The analysis lead to the installation of «Giredmet-911М1» (see the devil.1) or on the «Giredmet-1403М1» (see the devil.2). Extraction oven Assembly is shown in hell.30.

The outer crucible 4 sleep corundum with grain size of 50−100 µm to a height of 4−5 mm. Powder made from the material of the crucibles. The inner crucible 5 is inserted into the outer, between the walls of the crucible poured corundum powder.

The lower edge of the funnel 2 when installed in an extraction furnace should be 3−5 mm is omitted in the inner crucible. In the inner crucible download cut Nickel rod with a length of 25 mm and a diameter of 12 mm. the Crucible Assembly is mounted on a quartz stand inside 7 of the flask 1 and suspended from the funnel.

Heating of the material of the bath is initiated when the pressure in the extraction furnace is not more than 0,402 PA (3·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) Torr). The temperature was raised gradually to (900±50) °C to the temperature analysis in 10−15 min. At the temperature of analysis (table.2) the melt is degassed for 1−1,5 h to get the size of the corrections in the reference experiment ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 5·10% of nitrogen per 1 g of sample weight.

The definition of amendments the reference experiment carried out before analysis of each sample.

On the «Giredmet-1403М1» (see the devil.2) the amendment reference experiment is installed in the following order: not less than 5 minutes before the start of gas extraction from wet-process kiln 30 lead analytical system to its original position (valves 7, 13 are closed; 6, 9, 11 open; the valve 15 is open; the process of the oxidation furnace 10 is raised the Dewar vessel with liquid nitrogen); pump out the lock chamber the roughing pump; open the valve of the gateway is 1.5−2 turns; open the valve 7, close 6, 9, and include stopwatch; 15 close the valve with the gateway; after 10 minutes, close the valve 7, opening valve 6 and at the end of the separation process gas mixture (switch vacuum gauge in the «LT-2») measure the pressure of nitrogen automatic pressure gauge Mack-Leod 16; open the valve 9.

During the evacuation of gases from the analyzer through an airlock upload another sample, is pumped out of the gateway in fore-vacuum pump, then open the valve the gateway for 1.5−2 turns. At the end of pumping nitrogen from the analyzer, the device is ready for the next analysis (valves 6 and 9 are closed, 7 is open). Once you start the stopwatch the rotation of the handle gateway dropping the sample into the crucible and the gateway closed.

On the «Giredmet-911М1» (see the devil.1) the amendment of the control and experience is determined as follows: at least 5 minutes before the start of gas extraction from wet-process kiln 1 lead analytical system to its original position (valve 7 in the position of pumping, valve 16 and valve oxidizing furnace 11 is opened, valve 10 is closed, the process of the oxidation furnace is raised the Dewar vessel with liquid nitrogen); transfer valve 7 at position «pumping», close the valve 16 and include stopwatch; after 10 minutes, transfer valve 7 in the position of pumping and watching the end of the process of separation of gas mixtures according to the indications of the vacuum gauge systems; measure the nitrogen pressure gauge Mack-Leod 12; open the valve 16, pump out the nitrogen.

After the evacuation of gas from the analyzer unit is ready for next analysis.

Analysis of samples on the «Giredmet-1403М1» and «Giredmet-911М1» are in the same sequence as in the definition of amendments the reference experiment, and continue as long as the total mass of the analyte will not exceed the value specified in table.3.

Table 3


The analyzed material	Temperature of extraction, °C	Extraction time, min	The highest permissible ratio of the mass of the bath to the mass of the analyte	The mass of the analyte in a single crucible, g
Niobium, tantalum, vanadium and their alloys with chromium, tungsten and between	1800±50	10	10:1	3
Molybdenum, tungsten, rhenium and their alloys	1800±50	10	7:1	4
Zirconium and hafnium and their alloys	1800±50	10	25:1	1
Rare earth metals, yttrium and their alloys	1700±50	5	7:1	5

After the extraction of gas from each sample into the bath add 1 g of Nickel and degassed melt 3 min.

The process of the oxidation furnace during the whole time of operation in the mode of analysis remains immersed in the Dewar with liquid nitrogen.

Conditions analysis for specific materials are given in table.3.

4.4.2. Simultaneous determination of nitrogen and carbon in the powders of niobium and tantalum with particle size of 10−100 microns and an oxygen content of at least 0.07% (the mass fraction of nitrogen from 1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) to 3·10% carbon and from 1·10to 2·10%).

The analysis is carried out on the «Giredmet-911М1» or «Giredmet-1403М1» as specified in clause 4.4.1.

After measuring the pressure of nitrogen analyzer nitrogen is pumped and bring the temperature of the oxidizing furnace trap to -70 °C using chilled alcohol. Then measure the pressure of the carbon dioxide gas.

4.4.3. Determination of nitrogen in niobium, molybdenum, silicon pre-treatment of the sample surface (with a mass fraction of nitrogen from 2·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) to 2·10%)

Preparation of installation is carried out as specified in clause 4.1.1, oxidation of samples as specified in clause 4.3.2. The melt is degassed for 2−2,5 hours. the End of the degassing is characterized by the correction control experience at least 2 micrograms of nitrogen. The difference between two consecutive measurements amendments the reference experiment should not exceed 0.2 micrograms of nitrogen.

Analysis of niobium and molybdenum is carried out as specified in clause 4.4.1; for silicon:


the temperature of extraction	(1500±50) °C;
the extraction time	5 min;
the mass of the analyte material within the crucible	no more than 6 g.

4.4.2, 4.4.3. (Added, Rev. N 1).

4.5. Determination of hydrogen

Method of vacuum heating for the determination of hydrogen is as follows. The sample drop into the graphite crucible vacuum furnace, where at a temperature of ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1200 °C the decomposition of all hydrogen-bearing compounds of metals. Released at the same time in the gas phase, hydrogen is supplied to the analyzer where it is measured the pressure in a known volume.

4.5.1. Determination of hydrogen in niobium, the tantalum, vanadii, molybdenum, tungsten, Rennie, zirconium, hafnium, rare earth metals and their alloys, having a melting point ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) of 1200 °C, by vacuum heating (at a mass fraction of hydrogen is 2·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) %)

For analysis take the compact samples as well as samples of the powder and foil, pressed, as indicated in sec. 3. The analysis is carried out on the «Giredmet-911М1» (see the devil.1) or «Giredmet-1403М1» (see the devil.2). Instead of a stepped graphite crucible used thin wall with a thickness of the bottom and sides of 2 mm. Before analysis, the degassed crucible for 1−1. 5 h at a temperature of (1800±50) °C. the End of the degassing is characterized by exposures in the reference experiment ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) 1·10% of hydrogen in 1 g of sample weight of sample for 10 min at a temperature of (1200±20) °C.

The extraction time is 10 min. the Definition of amendments the reference experiment is carried out as specified in the PP.4.1.1 and 4.1.2. A distinctive feature is that in the analysis of the oxidation oven is disconnected from the analytical system. Analysis are in the same order as the definition of amendments the reference experiment. The process continues until, until the total mass of the analyte will not exceed 10 g.

5. PROCESSING OF THE RESULTS

5.1. Mass fraction of impurities ( ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) ) in percent is calculated by the formula

ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) ,

where ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) — pressure gas (co, N, H) in the volume of analyzer minus the pressure obtained in the determination of amendments reference experiment, PA (tor);

ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) — volume analyzer, cm;

— the mass of sample, g;

is a constant, equal in the calculation of the mass fraction of oxygen is 8.7·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) , carbon — 6,6·10, nitrogen — 1,5·10, and hydrogen — 1,

1·10 ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) .

5.2. Allowable absolute differences between the results of two parallel measurements at a probability ГОСТ 22720.1-77 Редкие металлы и сплавы на их основе. Методы определения кислорода, водорода, азота и углерода (с Изменениями N 1, 2) of 0.95 should not exceed the values given in table.4. For intermediate values of mass fractions of impurities permissible divergence is determined by linear interpolation.

Table 4


Determined by the impurity	Define mass fraction, %	Allowable absolute differences, %
Oxygen	5·10	5·10
	1·10	1·10
	2·10	1,5·10
	5·10	4·10
	1·10	5·10
	2·10	7·10
	5·10	2·10
	1·10	4·10
	2·10	7·10
	2·10	6·10
Carbon or nitrogen	1·10	1·10
	2·10	2·10
	5·10	4·10
	1·10	6·10
	5·10	2·10
	1·10	3·10
	1·10	2,5·10
	3·10	7·10
Hydrogen	2·10	1,2·10
	5·10	2,4·10
	1·10	4·10
	5·10	1,5·10
	1·10	3·10

(Changed edition, Rev. N 1).

5.3. Short characteristics method for the determination of impurities are given in table.5.

Table 5


Determined by the impurity	Method of determining impurities	The lower limit of detectable concentrations, %
Oxygen	The melting temperature of water (niobium, molybdenum, their alloys)	5·10
	Melting in Nickel bath	1·10
	Melting in a platinum bath	5·10
	Melting in the Nickel bath and the Nickel capsules	2·10
	Vacuumware high temperature without melting of the sample	2·10
	The melting temperature of water (fluorides of REE)	1·10
	Melting in a bath of fluoride REE	2·10
	The melting temperature of water (indium, gallium, and their alloys)	5·10
	Melting in the Nickel bath and the Nickel capsules with the use of tin	1·10
	Melting in the copper-Nickel bath	1·10
Carbon	Oxidative melting in vacuum	1·10
Nitrogen	Vacuum extraction in carbon-free melt of Nickel	2·10
Hydrogen	Vacuum heating	2·10

(Added, Rev. N 1).

GOST 22720.1-77

GOST 22720.1−77 Rare metals and alloys on their basis. Methods of determination of oxygen, hydrogen, nitrogen and carbon (with Amendments No. 1, 2)

2. APPARATUS, REAGENTS AND SOLUTIONS

3. PREPARATION FOR ASSAY

4. ANALYSIS

5. PROCESSING OF THE RESULTS

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GOST 22720.1-77

GOST 22720.1−77 Rare metals and alloys on their basis. Methods of determination of oxygen, hydrogen, nitrogen and carbon (with Amendments No. 1, 2)

2. APPARATUS, REAGENTS AND SOLUTIONS

3. PREPARATION FOR ASSAY

4. ANALYSIS

5. PROCESSING OF THE RESULTS

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